HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Ethanol → 4-(9-cyclopentyl-5,7,7-trimethyl-6-oxo-6,7,8,9-tetrahydro-5H-pyrimido[4,5-b][1,4]diazepin-2-ylamino)-3-methyl-benzoic acid
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Ethanol | HCID 702 | — |
| Edukt | 4-Amino-3-methylbenzoic acid | HCID 75598 | — |
| Edukt | 2-Chloro-9-cyclopentyl-5,7,7-trimethyl-5,7,8,9-tetrahydro-pyrimido[4,5-b][1,4]diazepin-6-one | HCID 59295116 | — |
| Katalysator | Hydrochloric Acid | HCID 313 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Produkt | 4-(9-cyclopentyl-5,7,7-trimethyl-6-oxo-6,7,8,9-tetrahydro-5H-pyrimido[4,5-b][1,4]diazepin-2-ylamino)-3-methyl-benzoic acid | HCID 68903247 | 41,6% |
Reaktionsschritte
A mixture of 0.0398 g (0.00013 mole) of 2-chloro-9-cyclopentyl-5,7,7-trimethyl-5,7,8,9-tetrahydro-pyrimido[4,5-b][1,4]diazepin-6-one (VII-38), 0.022 g (0.000143 mole) of 4-amino-3-methylbenzoic acid, 0.7 mL of ethanol, 2.8 mL of water and 3 drops of hydrochloric acid was heated at reflux for 17 hours. The mixture was cooled, and the white precipitate that formed was collected by filtration to give 0.0229 g of 4-(9-cyclopentyl-5,7,7-trimethyl-6-oxo-6,7,8,9-tetrahydro-5H-pyrimido[4,5-b][1,4]diazepin-2-ylamino)-3-methyl-benzoic acid (I-56a) as a white solid.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07517873B2 |
| Quelldatensatz | uspto-grants-2009_04 |
| ORD ID | ord-720d3c121b604c31bf430582bcd0fa3e |
| Quellennotiz | uspto-grants-2009_04 |